Continuous separator



Oct. 27, 1953 L. KASEHAGEN CONTINUOUS SEPARATOR 3 Sheets-Sheet l Filed June 17, 1948 hm] mm -R. w m n QN N G E Y In W T 1 .M G K I 55 -Ebzm L u 55 W EMIUE wm zmwo 5E: mm @UUIO www) mOmmmm-a EOU oct. 27, 1953 l.. KASEHAGEN 2,656,895

CONTINUOUS SEPARATOR Filed June l?, 1948 `3 Sheets-Sheet 2 /coMPRcssEo AIR 64 3|/ 54 53 5e l iff.

r T T mv 53 6| 59 Fig. 2

Leo Kosehogen, INVENTOR.

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ATTORNEY Oct.4 27, 1953 Filed June 17, 1948 L. KASEHAGEN CONTINUOUS SEPARATOR .3 Sheets-Sheet 3 Leo Koseho gen, INVENTOR.

ATTORNEY Patented Oct. 27, 1953 CONTINU UUS SEPARA'IOR YLoo ,Kaschasem .West Chester. Paf. ,assignor .to Atlas Iowdor Company, Wilmington, Dol... .o

corporation of Delaware Application June V:17, 1948, `SerialiNo.ll ;559

(Cl. 183f?2.7,)

2 `Claimsi-'Lhe :present invention relates vto a continuous separator.

:An object of the invention is to ,provide an improved `device rior oo ntinucuisly 4separat-ing a gas and arslurry-of solid material Ain .a liquid occurringin admixture.

A .more specific object .is ,to Yprovide an improved device for continuously separating hydrogen :sas and .zo @slurry `of `sumwrtod hydrogenation Qatalyst .in a polyhydric A alcohol so lution `occurring -in admixture as ,the reaction mix-turc leaving a high -pressure continuous sucarA-hydlogenatonsystem 4 A furt-,her L object `is to V,provide a continuous separator of the `class referred to which Aembodies improvodgslur ylevelregulatingrand-slurry discharging elements.

A still further object is to provide .a `conti-nuous separator vof lthe class .referred to which embodies .improvedslurry .level indicating means.

SI1-ho above and other objects will become apparent in theoourse ,of the .following description.

In the drawings, wherein .like :numerals .refer to oorrespondiosparts,

Eigure ,1 a `iiovv sheet l of a continuous `sugar hydrogenatns plant :illustrating vda grammatically the continuous separator and alliedequipmont- .Eigure ,2 Ais .an enlarged ,and pmore detailed diagrammatic ,illustrationiof ,the continuous separatorand allied equipment.

Figure 3 is a vertical cross section of the .separator vessel.

`Eigure 4 is ,a `horizontal section through the f separator ,taken on the line 4.-4 of Figure-3.

Referring f now .to Vrieure l, a dry 4reduoilole Sugar, such as glucose, and water are introduceclinto the mixing tank l in proportions to prepare 3. solution of predetermined Concentration, .for.example50%. Bump Il advances 4the sugarsolutionfrom mixing .l0 -to the storavso tank el2 where a selected `proportion of hydrosenating catalyst is :addod- The tanks l0 and I 2 are both conventon'alprocess tanks Vpro-- vided with .agitators to keep .the contents homosenoous- The catalyst preferred `for sugar hydrogenation is a conventional reduced nickel catalyst .supportedon diatomaceous. earth. When mixed .With the `sugar `solution in tank L2 .the catalyst is suspended, forming a slurry.

The `slurry .of catalyst in `sugar solution is Dumped bythe pump ,i3 `through .a `Dreheater M .to warm the slurry, Iand Ainto the variable dflfely .-Dllml J5 lwhich .ffoeds .the :slurry into the bottom of a rstautoclave :t6 .at a selected rate. l 'Ilic autoclave t6 and `succeeding `autoclaves aregmaintained at ahydrogenating temperature, 'to 165 C. for producing sorbitol from glucose, by steam jacketing or other conventionalheating means.

Hydrogen for the process is `introduced into the lower part of Athe autoclave 1 6 at 'hydrogenating pressure, 'suitably 4from 1 000` to 52000 pounds per ,square linch causo, from a circulating systcrxi .to Abe described hereinafter The hydrogen -is-preferably introduced through a perforated nozzle |51 (shown vin `dotted line). The charge of slurry fand hydrogen pass upwardly through the autoclave 116, and pass out at the upper end Vthereof through a pipe I8 and into the lower -part of the second -`heated `autoclave I9. :Bassing 4upwardly through theiautool-aye I9 the-charge leaves .fthroughv'the pipeZDand enters the ilower part of the third vheated autoclave '2|. Three autoclaves are illustrated but it will be understood that for the purposes of the `invention oneror any largernumber ofautoolaves can hoomployed.

From fthe top of `the --third autoclave 42l the reaf-ctionmixture, which at :this time Aconsists of unreacted hydrogen 4gas `and a slurry of spent catalyst in the solution of polyhydric alcohol, here sorbitol, :in water passes through a pipe '212 zto the separator designated `genera1ly=by the numeral T23. `Inthe separator `2 3 the reaction mixture is continuously .separated into Ifractions consisting respectively of -the hydrogen `gas and the slurry. flfheslurry leaves the bottom -of the sepol'otori rthrough the discharge line 24, passes through -the fproduct =coo1er 25, discharge and pressure reducing valve '2 6 and into fthe produot freceiver ,2.1. The cooled slurry, at atmos- Rhorio pressure, is VWithdrawnfrom time to time from the receiver l2-1 and 4treated by conventiona1 product recovery steps including nitration to Y remove 1thespent catalyst.

Iglydrogen gas leaves .the separator through the line A2,8 and ,passes to a Condenser `consist-- ing of o gas cooler 2 9 and a solvent separator 3 0 ior -the purpose of condensing and removing A4'sugar solvent, lhere water, from `the hot .hydrogen gas. f Condensed,solvent leaves the separator 3 0 through the `solvent return line 3| which enters 'the ,lower portion of the separator 2 3. Hydrogen gas leaves vthe solvent separator 30 `fby the 1in e.;32 connected to the low pressure Side .of the-circulating compressor 353.. The circulating compressor, in the-illustrated form of the ianoorotus, runs at constant speed and is provided with a `'by-pass controlled by the throttle valve 34 for the purpose of permitting the maintenance of a selected rate of flow into the reactors. Hydrogen from the compressor 33 passes through an orifice flow meter 35 and preheater 36 and so into the iirst autoclave I6 through the nozzle I1. The throttle valve 34 can be controlled either manually, or Aautomatically by conventional means, to maintain the selected rate of flow in accordance with the measurements of the meter 35.

Hydrogen is initially introduced into the system, and make-up hydrogen periodically added to the system, from the low pressure gas storage tank 31, compressor 38, high pressure gas storage bottle 39, and regulating valve 40. When the system reaches its normal operating state hydrogen replacing that chemically reacted with the sugar and any process losses is automatically introduced from the high pressure storage bottle 39 by the operation of the regulating valve 4U which is set to admit hydrogen to the circulating Isystem to maintain the selected gas pressure.

In the system illustrated, the rate of feed of the sugar and catalyst slurry can be varied by adjustment of the variable delivery pump I5. The rate of hydrogen feed can also be varied by the setting of the throttle valve 34.

In the operation of the hydrogenation plant illustrated in Figure l a large excess of hydrogen is employed over the amount required to combine chemically with the sugar. The amount of the excess for preferred operation is described and claimed in my copending application, Serial No. 32,845, led June 14, 1948. The apparatus which is the subject matter of the instant application is particularly useful for the preferred operation, but is not limited to use therewith.

The reacton mixture leaving the last autoclave 2I is at reaction pressure and this pressure must be maintained on the free hydrogen so that it can be recycled through the system. The slurry must be removed from the system continuously and dropped down to atmospheric pressure for working up to the final product. Several problems arise in separating and discharging this slurry due to its physical nature, the pressureV involved, and the continuous manner in which it is delivered for discharge. Aibody of the slurry must be maintained as a pressure seal in the separator 23 and the discharge line 24. On the other hand, the slurry must be discharged as rapidly as it arrives to prevent fouling of the hydrogen recycling system and the destruction of the circulating compressor 33 and allied equipment. The slurry contains the relatively heavy catalyst in suspension and requires special provisions for preventing settling of the catalyst and for indicating and regulating the slurry level in the separator 23.

Referring now to Figures 3 and 4, the separator 23 is a vertically disposed elongated vessel with a horizontal cross section relatively small with respect to its capacity. The upper end of the vessel provides a hydrogen gas receiving portion and the lower end provides a slurry receiving portion. Reaction mixture from the line 22 enters the separator 23 through the tangential nozzle 59 in the upper part of the vessel impinging against a wier plate I and receiving a swirling motion. The slurry then falls to the lower end of the separator 23 striking the bailie 52 which directs the flow away from the level indicating floats 53 and 54. The inside dimensions of the separator are such that there is turbulence and rapid ow of slurry which prevents settlingof the suspended catalyst. Slurry leaves the lower end of the separator 23 through the outlet 55 which is connected to the discharge line 24 (Figs. 1 and 2). Hydrogen leaves the upper end of the separator 23 through the outlet 56 which is connected to the line 28 (Figs. 1 and 2) As illustrated in Figure 2 the separator 23 is .provided with a reflex type liquid level sight glass 51 the upper connection 58 communicating with the interior of the separator vessel above the normal slurry level and the lower connection 59 communicating with the interior of the separator vessel below the normal slurry level. Due to the fact that liquid in the separator 23 is a slurry, a conventional sight glass would not work because the suspended catalyst would settle out and block the lower connection 59 and also because the catalyst would deposit on the sight glass tube and render it opaque in a short time. The sight glass 51 is made practical in this device by bringing the solvent condensate, stripped from the hydrogen gas in the cooler 29 and separator 30, through the solvent return line 3| to the lower end of the sight glass and connecting the line 3l to the lower connection 59. By this means clear, condensed solvent (Water or other sugar solvent) flows continuously into the separator and constitutes the indicating liquid in the sight glass 51. The glass 51 remains clear and gives a readily observable indication of the slurry level in the separator 23. The solvent has a lower specific gravity than the slurry and therefore the liquid level in the sight glass 51 is always proportionately higher than the slurry level in the separator 23.

lThe operation of the slurry discharge valve 26 is automatically controlled by conventional means, linking the iioat 53 through a float position responsive pneumatic controller 6G to the pneumatically operated diaphragm valve motor 6I and valve positioner 62. The valve motor 6I and positioner 62 are likewise conventional items of manufacture. Other types of automatic devices for operating the valve 26 can obviously be employed.

The successful operation of the float 53 in the slurry is due to the construction of the separator which maintains the catalyst suspended and provides a homogeneous flowing body of slurry.

To provide protection for the hydrogen circulating system against the possibility of failure of the valve 26 to discharge slurry a second oat 54 is positioned in the separator 23 above the float 53 so that a rising level of slurry will raise the float 54. A second float position responsive.

pneumatic controller G3 is operatively connected to the float 54 so that if the latter is raised by the slurry a pneumatically actuated switch 64 is operated. The switch 64 can sound an audible alarm and/or stop the circulating compressor 33 and the slurry feed pump I5.

In the operation of the continuous separator of the invention the reaction mixture is allowed to enter the separator 23 through the nozzle 59. The gaseous hydrogen fraction of the mixture is returned to the circulating system after being stripped of Ventrained sugar solvent in the gas cooler 29 and separator 30. The slurry fraction of the mixture falls to the slurry receiving lower portion of the separator 23. As the liquid level rises the float 53 is raised and when it reaches a predetermined level the controller 60 actuates the valve operating motor 6| and valve positioner 62 to open the discharge valve 26. The valve 26 is thereafter opened or closed as required by the setting of the controller 60 in response to the position of the float 53 and hence the level of the slurry. This arrangement provides for maximum eniciency of the separator, for preventing pressure changes within the hydrogenatingautoclaves, and protects the hydrogen circulating system from contamination with slurry.

It will be apparent that the apparatus described herein and claimed hereafter is adapted for use in other systems and that many modifications can be made Without departing from the invention.

What is claimed is:

1. A device for continuously separating a gas and a slurry of suspended solids in liquids from a mixture thereof, comprising a vertically disposed separator having in its upper portion an inlet for the mixture to be separated and further having a gas outlet above said inlet and a slurry outlet in the lower portion of the separator, a condenser connected to the said gas outlet to condense vapor picked up by the gas from said slurry, a liquid level sight glass disposed outside of said separator and having a lower connection communicating with the lower portion of the separator and an upper connection communicating with the upper portion of the separator, and a liquid conduit connecting the said liquid condenser and the said lower connection of the liquid level sight glass whereby to return condensed liquid to the slurry and to provide a supply of clear condensed liquid to the said sight glass to function as a visible indicator of the level of slurry in the said separator.

2. A device for continuously separating liquid and gas at high pressure comprising a vertically disposed separator having a horizontal cross section which is small relative to its capacity, said separator having an inlet disposed substantially tangentially in the upper portion of the separator, said separator having a liquid outlet in its lower portion and a gas outlet in its upper portion above References Cited in the le of this patent UNITED STATES PATENTS Number Name Date 1,499,710 Weisgerber July 1, 1924 1,619,919 Cook Mar. 8, 1927 1,834,180 Raymond Dec. 1, 1931 2,353,833 Kimmell July 18, 1944 2,419,275 Metzgar Apr. 22, 1947 2,419,300 Tollefson Apr. 22, 1947 2,421,451 Balcar June 3, 194'? OTHER REFERENCES Publication: Chem. Eng. Catalogue, 1942-43; page 661. 

